A kind of tetranuclear copper complex and its preparation method and application
A technology for copper complexes and complexes, applied in separation methods, pharmaceutical formulations, organic chemical methods, etc., can solve problems such as pollution, and achieve the effect of simple preparation methods
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[0037] The invention provides a method for preparing the tetranuclear copper complex, comprising the following steps:
[0038] (1) mixing substituted phenol, lead acetate and dehydrated alcohol to obtain a mixed solution;
[0039] (2) After mixing the mixed solution with anhydrous methanol solution of N,N-bis(3-aminopropyl)-2-pyridinemethylamine, carry out a coordination condensation reaction to obtain a lead complex;
[0040] (3) Under alkaline conditions, the lead complex and the anhydrous methanol solution of copper sulfate are mixed and then subjected to a displacement reaction to obtain the tetranuclear copper complex;
[0041] The substituted phenol is 2,6-diformyl-4-methylphenol, 2,6-diformyl-4-methoxyphenol, 2,6-diformyl-4-fluorophenol, 2,6 - Diformyl-4-chlorophenol or 2,6-diformyl-4-bromophenol.
[0042] In the present invention, the lead acetate in the step (1) is preferably lead acetate tetrahydrate.
[0043] In the present invention, the molar ratio of substitut...
Embodiment 1
[0075] Mix 0.5mmol of 2,6-diformyl-4-methylphenol, 0.5mmol of lead acetate tetrahydrate and 15mL of absolute ethanol and stir at 300rpm for 2h to obtain a mixed solution; The 10mL anhydrous methanol solution of (3-aminopropyl)-2-pyridylmethanamine is added dropwise in the mixed solution at a speed of 3 drops / second, and after the dropwise addition, the solution turns from bright yellow turbidity to a yellow transparent solution, at 300rpm Stir at a speed of 100°C to carry out the coordination condensation reaction, and obtain the lead complex after 3 hours; then add 15 mL of anhydrous methanol solution containing 1.3 mmol copper sulfate pentahydrate to the lead complex dropwise at a rate of 3 drops / second, and the dropwise addition is completed Afterwards, the solution becomes light green and turbid, and triethylamine is added dropwise to adjust the pH value to 8.5, and the replacement reaction is carried out with stirring at a rotating speed of 300 rpm. After stirring for 4 ho...
Embodiment 2
[0091] Mix 0.4mmol of 2,6-diformyl-4-bromophenol, 0.6mmol of lead acetate tetrahydrate and 14mL of absolute ethanol and stir at 200rpm for 2.2h to obtain a mixed solution; (3-Aminopropyl)-2-Pyridylmethylamine 8mL anhydrous methanol solution is added dropwise in the mixed solution at a speed of 2 drops / second, after the dropwise addition, the solution turns from bright yellow turbidity to a yellow transparent solution, at 200rpm Stir at a speed of 100°C to carry out the coordination condensation reaction, and obtain the lead complex after 3.2 hours; then add 12 mL of anhydrous methanol solution containing 1.4 mmol of copper sulfate pentahydrate to the lead complex dropwise at a rate of 2 drops / second, and dropwise add After completion, the solution turned light green and turbid, and triethylamine was added dropwise to adjust the pH value to 8.5, and stirred at a speed of 200rpm to carry out the replacement reaction, and after stirring for 3.5h, filter it with a sand core; use 28...
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